Process for the purification of alcohol and similar liquids.



E. GUILLAUME.

PROCESS FOR THE PURIFICATION OF ALCOHOL AND SIMILAR LIQUIDS. APPLIOATIONFILED APR. 1;, 1907.

' 992,498, Patented May 16; 1911.

s SHEETS-SHEET 1i WITNESSES: \NVENTOR,

Emma QmLLAuME,

E. GUILLAUME. moorss FOR THE PURIFICATION OF ALCOHOL AND IMI AR LIQUIDS.

APPLIGATION FILED APR.11, 1907. 992,498, Patented'May16,191l.-

3 SHEETS-SHEET 2.

WITNESSES- mvsmm I I ENHLE GU\LLP\UME,-

ATT DRNEY.

v E. GUILLAUME. PROGESS PORTHE PURIFICATION OF ALCOHOL AND SIMILARLIQUIDS.

' APPLIOATION FILED APR.11, 1907.

992,498. r I PatentedMy-w, 1911.;

3 SHEETS-SHEET 3-.

- v )NVENTOR.

" [EgglLE GUILLAU E,

' Attorgg UNITED STATES PATENT OFFICE.

I EMILE GUIIrLAUME, 0F ZBIiIDA, ALGERIA. PROCESS FOR THE PURIFICATION OFALCOHOL AND SIMILAR LIQUIDS.

Specification of Letters Patent. Patented May 16, 1911.

Application filed April 11, 1907. Serial No. 367,697.

To all whom it may concern:

Be 1t known that I, Emu: GUILLAUME', a citizen of France, resldlng atAvenue de la (xare, Bhda, Algeria, have invented new and usefulImprovements in Processes for the Purification of Alcohol and SimilarLiquids,

(for which I have obtained a patent in France, No. 365,417, bearingdateof April 19, 1906, and Canada, No. 102,111, November 20, 1906,) of whichthe following 1s a spoolfication.

My invention relates to a new and 1mproved process for the purificationof alcohol and similar liquids.

It relates particularly to a continuous rocess for removing in oneoperation and 111 one combined apparatus the impurities mixed with thealcohol under the name of head and tail .products, whereby there isobtained, as the final product, a pure alcohol of very high degree, 99%,the other 1% being water and sllght traces of other impurities.

It relates, further, to a process in which there are obtained in oneoperation two grades of alcohol, the one having a high quality suitablefor many technical urposes, and the other, an alcohol of the highestattainable purity. The first grade amounting, for example, to aboutone-half the total uantity obtained. is drawn o'fi' from one 0 the uppershelves of the rectifymg column in the form of ethyl alcohol practicallyfree from head product-s, but containing a small quantity of the mostvolatile tail products. The second portion passing from the top of thedephlegmator, or condenser. into the purifying apparatus, consists ofethyl alcohol carrying head products. It is from this second portionthat the ethyl alcohol, free from head products, is

obtained almost absolutely pure.

By head products are meant those impurities having a lower boiling pointthan ethyl alcohol: by tail products, those impurities whose boilingpoint is higher than ethyl alcohol. Under head products may be includedthe aldehydes, ,ethers, and the like, while the tail products 'includesuch impurities as amyl alcohol, isoamyl acetate,

isovalerate of ethyl, etc.

My process is not limited to any specific apparatus, and that shown inthe drawing is only by way of example.

In the drawings :-Figur'e 1 shows'a simple form of apparatus, but one inwhich my results.

' pipe 11 controlled by the rocess in its entirety can be carried out:ig. 2 is an approved form, and Fig. 3, another modification which givesthe best I have chosen as an example a rectify when of'properdimensions,

of producing, per '24 hours, 2500 hectoliters of alcohol including thewater combined therewith. Such a column would contain approximately 45to 50 plates, would have a diameter of 1.6 meters and be about 7.5meters high.

Referring to the drawings, particularly to Fig. 1, 1 is a rectifyingcolumn carrying a series of perforated plates, such as are found in anyordinary rectifying column; C the condenser, or dephlegmator, toppingrectifying column 1, and connected by the pipe 12., controlled by thecock 5,'with the two-part purification column 67. From one of the uppershelves, here shown as the fifth from the top, a ipe 7o", controlled bycock 2, leads to the coi p of the refrigerator 3, and thence to thetestingjap aratus 4. From the base ofthe column 6- a pipe 8 leadsthrough the coil f-,-of refri erator 3, into the pipe f and the tester9. bove the column 6-7 is located a condenser 18, connected therewith bythe pipe-k 17 is a supplementary condenser, or refrigerator, connectedto the condenser 18 by the pipe h and to the refrigerator 3 by the cook12.

Water for cooling the condensers enters the refrigerator 3 by the pipeW, and follows the course of the pipes W, refrigerator 17, pipe -Wrefrigerator 18, pipe W, con.- denser 'O and pipe W In Figs. 2 and 3,the water follows the pipes W to W.

To operate my process, I proceed as follows, referring first to Fig. 1.Into the rectifying column 1 at the bottom, I introduce as raw material,an alcoholic product which has refer-ably been previously distilled toraise its percentage of alcohol to 50%, for example. I raise thetemperature of the product during treatment in the rectifying columnabove the boilin point of ethyl alcohol, say to 80 C. T e vapors,composed of'ethyl alcohol, head products, and the most volatile of thetail products, rise through the rectifying column 1 into the condenserG, where, in order to strengthen them, they are cooled off and partiallycondensed. From the condenser the condensed vapors, at a temperature ofeeaae 7 580 (3., flow down on to the plates of the I low 757 8 C. andtraces of the head prodrectifier, and in flowing down meet an ascendingcurrent of weak alcoholic -va ors; the products are thereby brought to e1111 1- tion and evaporation and become richer in alcohol. These arecondensed and deposited on the shelves p, and by frequent repetition ofthis operatlon a very strong alcohol is finally obtained. The hquidcondensed on the upper shelves of the rectifying column is composed of97% to 98% ethyl alcohol, water Q and the most volatile of the tailproducts, with small traces of the head products (ll-200000th circa),composed of the aldehydes and light ethers. The tail products,

carried by the alcoholic liquor on theshelves, are traces of amylalcohol and several of the most volatile of the tail products, such as,for example, the isobutyrate of ethyl. From one of the upper shelves ofthe restifying column, at a point where the alcohol is nearly free fromthe tail products, I draw off the alcohol deposited thereon. I haveshown the drawing oif as taking place at the fifth plate from the top,though the choice would be determined by the quality of the liquiddesired. In practice, tap cocks, connecting the pipe p with several ofthe upper plates would be employed. From the shelf chosen, the liquidflows through the pipe 32', controlled by the cock 2, through therefrigerator 3, to the tester 4' and to the proper storage receptacles.

The operator tests the quality-of the alcohol in t by either taste,smell, or chemical analysis. Smell is the test most readily employed,and the aldehydes and the ether being very pungent, they will make knownthe presence of head products. If the operator detects any considerablequantity of head products in the tester 4, he will know that he isdrawing off the liquor too rapidly from the shelves, and will close moreor less the valve 2, or else he will increase the heat in the rectifyingcolumn.

The second portion of the vapors, not condensed on the shelves 1?, andconsisting of ethyl alcohol and head products, in the proportion ofcirca 99% alcohol and circa 1% aldehyde and ether, with a possibleinfinitesimal amount of tail products, passes from the top of thecondenser C through the pipe 7:. into the middle portion a of thepurification column 6-7. Here the ethyl alcohol is condensed on theplates of the column 6, and is drawn oil as almost absolute alcohol bythe pipe 8 through the refrigerator to the tester 9, and thence to,storage. The head products pass upward through the column 7, pipe hcondenser 18, pipe 71. to refrigerator 17, whence the condensed productspass by pipe 14, to the refrigerator, and to the tester 13. Should thetemperature in column 6-7 become too low, (that is, be-

products.

ucts show themselves in the tester 9, the heat applied at the base ofcolumn 6, in a closed coil, is increased by means of additional steamthrough 10, c and e, which causes a revaporization and driving off ofthe contained head products. The columns 6-7 are formed like column 1,the action of the shelves being the same in each.

I have thus carried out my process, obtaining one grade of alcohol fromthe shelves, and an almost anhydrous alcohol from the base of column 67.

The condensers 18 and 17 are provided at their'tops with pipes c and eto allow the pressure therein to remain approximately equal to that ofthe atmosphere. The finally condensed head products from the condensers18 and 17 pass by the pipes 15 and 14 through the pipe 11 into therefrigerator and tester 13.

The modification shown in Fig. 2 diti'ers only slightly from theapparatus in Fig. 1, but gives better results. In this I do not drawofi? the first portion of the alcohol (that is to say the portioncontaining the most volatile tail products and ethyl alcohol) from theupper plates of the rectifying column, but I arrange between thecondenser of the said column and the column of final purification, anintermediate column, into which I send the alcoholic vapors leaving thetop of the condenser of the rectifying column, and from the bottom ofthe said intermediate column, I draw off an alcohol corresponding tothat drawn ofl" from the shelves of the rectifying column in Fig. 1, butof a higher quality. In this modification the heated alcoholic vaporsare compelled to rise over the shelves ofrectifying column 1, into thecondenser C, some being condensed and flowing back again into column 1,as in Fig. 1. The vapor passing out of condenser C through the pipe h,controlled by valve 5 contains the most volatile tail products, whichhave not been left on the shelves of column 1 and in the condenser C,together with ethyl, alcohol and head These vapors pass into the base I)of the column 20C (similar in construction to 1-0 of Fig. 1) and ascendthrough the analyzer (reflux condenser) 20 into the condenser C. Intheir passage over the plates in 20 and in the condenser C, a portion ofthe ethyl alcohol and the tail products become condensed and fallto thebase I), whence by the pipep' they are drawn, through the coil p of thecondenser 3, to

pipe p tester 4, and storage receptacles.

- 72., pass to the nal purification column 6-7,

thence to the condensers l8-l7 and the refrigerator 3, as in Fig. 1, thepurified alcohol being drawn off through pipe 8 to the refrigerator andthe storage receptacles.

In the modification shown in Fig. 3, the ethyl alcohol carrying headproducts, with the most volatile tail .products, passes off at the topof condenser C, through the pipe h to the portion 6 of the purifyingcolumn 22-20, constructed and operating the same as column 6-7, of Fig.1, the purified ethyl alcohol, corresponding to that drawn off from theshelves of 1, Fig. 1, being led from I the base of column 22, throughthe refrigerator coil to the tester 4 and-storage rece tacles. Thisethyl "alcohol isevidently st1ll purer than that drawn off from the baseofcolumn 20, Fig. 2,'since it has been subjected to the purifying actionof the double column 22-20, instead of the single column 20. The ethylalcohol and head products that are uncondensed pass from column 2022 tothe column of final purification 67 where the ethyl alcohol parts withpractically all traces of head products, and is drawn off as absolutelypure ethyl alcohol from the base' of column (3,by the pipe 8, to therefrigerator, the tester 9, and storage receptacles. What uncondensedheadproducts enter the condensers '18 and 17, become condensed thereinand pass from 17 to the tester 13, this part of the operation beingthe-same in all the figures.

The cocks 5 in Figs. 1, 2, 3, and 21 in Fig. 3 control the amount ofhead products passing over with the ethyl alcohol, since if the operatordetects the odor of head products in the final'products, he closes thecooks and subjects the vapors passing from the condensers to moreintense treatment before they leave the same.

Having thus fully illustrated and described my invention, what I claimis 1. The process of rectifying and purifying previously distilledalcohol, which consists in subjecting the same in a rectifying column toheat sufficient to cause it to vapo rize and a predetermined portionthereof to become condensed, in the form of ethyl alcohol with trace oftail products, upon the upper shelves of the rectifier, drawing off tothe refrigerating device the alcohol thus collected, passing theremaining portion of the products of the rectifier issuing from the topof the rectifying column in the form of ethyl alcohol and head productsthrough a' final purification device, separating therein the ethylalcohol from the head products and drawing off the alcohol in the formof almost absolutely pure ethyl alcohol, and then condensing and drawingoff the'head products, substantially as described.

2. The process of rectifying and purifying alcohol, whichconsists insubjecting the same to heat suflicient to cause it to vaporize and risein the rectifying column and become condensed on the upper shelvesthereof in the form of ethyl alcohol carrying traces of tail products,controlling the rectification in such a manner that practically half ofthe products of the column are drawn off from the upper shelves, passingthe remaining half of the rectifier products as ethyl alcohol and headproducts to a final purification device, condensingtherein the alcoholicvapor and separating the alcohol from the head products, drawing off thealcoholin the form of almost absolutely pure ethyl alcohol, andseparately condensing and collecting the head products, substantially asset forth.

3. The process of rectifylng and purifying previously distilled alcohol,which consists in subjecting the same in a rectifying column to heatsufiicient to cause it to vaporize and pass out of'the top of thecondenser inthe form of ethyl alcohol, head products and a trace of tailproducts, leading these vapors into the bottom of an intermediatecolumn, condensing therein a certain part of the alcohol vapors, drawingoff the condensate to the refrigerator in the form of a Very pure ethylalcohol containing only traces of tail products, passing the uncondensedethyl alcohol and head products to the column of final purification, andtherein separately condensing the head products and the ethyl alcohol,and drawing offthe alcohol in the form of almost absolutely pure ethylalcohol substantially. as set forth.

4. The process of rectifying and purifying previously distilled alcohol,which consists in subjecting the same in a rectifying column toheat'sufiicient to cause it to vaporize and pass out of the top of thecondenser in the form of ethyl alcohol, head products and a trace oftail products, leading these vapors into an intermediate therein acertain part of the alcohol vapors, drawing oil the condensate to therefrigerator in the form of a very pure ethyl alcohol-v containing onlytraces of tail products, passing the uncondensed ethyl alcohol and headproducts to the column of final purification, and therein separatelycondensing the head products and the ethyl alcohol, and

drawing off the alcohol in the form of almost absolutely pure as sethforth. fy

5. T e process of recti in and urif in alcohol, which consists insubjedting th same in a rectifying column to heat suflicient to cause itto vaporize and pass out of the top of the condenser in the form ofethyl alcohol, head products and a trace of tail products, leading thesevaporsinto the bottom of an intermediate column, condensing therein acertain part of the alcohol vapors, drawing off the condensate to therefrigerator ethyl alcohol, substantially column, condensing in the formof a very pure ethyl alcohol containing only traces of tail products,passing the uncondensed ethyl alcohol and head products to the column offinal purification,

and therein separately condensing the head products and the ethylalcohol, and drawing off the alcohol as almost absolutely pure ethylalcohol, substantially as set forth.

comes EMILE GUILLAUME.

Witnesses;

JULEs FAYOLLET, EUGENE PIOHON.

